(2,2-Diethoxyethyl)dimethylamine → HCID 131711015, 화합물

HRID 1833420노트

반응식

HRID 1833420 반응식
[CH2:1]([O:3][CH:4]([O:9][CH2:10][CH3:11])[CH2:5][N:6]([CH3:8])[CH3:7])[CH3:2].[N+:12]([C:15]1[CH:20]=[CH:19][C:18]([C:21]2[O:25][C:24]([C:26]([CH2:28][Cl:29])=[O:27])=[CH:23][CH:22]=2)=[CH:17][CH:16]=1)([O-:14])=[O:13]>C(O)C>[OH2:3].[Cl-:29].[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][N+:6]([CH3:7])([CH3:8])[CH2:28][C:26]([C:24]1[O:25][C:21]([C:18]2[CH:19]=[CH:20][C:15]([N+:12]([O-:14])=[O:13])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1)=[O:27])[CH3:11].[CH2:10]([O:9][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][N+:6]([CH2:28][C:26]([C:24]1[O:25][C:21]([C:18]2[CH:19]=[CH:20][C:15]([N+:12]([O-:14])=[O:13])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1)=[O:27])([CH3:7])[CH3:8])[CH3:11].[Cl-:29]

참가 물질

4

반응물 2

HCID 77163(2,2-Diethoxyethyl)dimethylamineHCID 213893612-Chloro-1-[5-(4-nitrophenyl)furan-2-yl]ethan-1-one

생성물 1

HCID 131711015HCID 131711015, 화합물수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Dimethylaminoacetaldehyde diethyl acetal (29 g, 0.18 mole) was added dropwise to a stirred mixture of 40 g (0.15 mole) of chloromethyl 5-(4-nitrophenyl)-2-furyl ketone in 750 ml of absolute ethanol at 30° over 15 minutes. The mixture was heated under reflux for 22 hrs and was filtered hot to remove a black insoluble material. The filtrate was cooled in ice, and the brown solid was filtered and discarded. The filtrate was diluted with 1.5 liters of anhydrous ether, and the solid which was deposited was collected by filtration to give 45 g (69%) of (2,2-diethoxyethyl)dimethyl[5-(4-nitrophenyl)-2-furoylmethyl] ammonium chloride hemihydrate. Two recrystallizations from CH3CN gave an analytical sample, m.p. 113°-118°.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 22 hrs
  3. filtrationwas filtered hot
  4. customto remove a black insoluble material
  5. temperatureThe filtrate was cooled in ice
  6. filtrationthe brown solid was filtered
  7. additionThe filtrate was diluted with 1.5 liters of anhydrous ether
  8. filtrationthe solid which was deposited was collected by filtration

출처 및 근거

ORD 기록
ord-3f0a2f3dd4d74a18ab0a46df57df333f
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04066671

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